Literature DB >> 21580120

Bis(2,4,6-triamino-1,3,5-triazin-1-ium) hydrogen phosphate trihydrate.

Xue-Mei Li, Si-Si Feng, Fan Wang, Qi Ma, Miao-Li Zhu.   

Abstract

In the title hydrated mol-ecular salt, 2C(3)H(7)N(6) (+)·HPO(4) (2-)·3H(2)O, three of the O atoms of the hydrogen phosphate anion are disordered over two positions, with relative occupancies of 0.763 (1) and 0.237 (1). In the crystal, the components are linked by N-H⋯N, N-H⋯O and O-H⋯O hydrogen bonds.

Entities:  

Year:  2009        PMID： 21580120      PMCID： PMC2980075          DOI： 10.1107/S1600536809054798

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For related structures, see: Choi et al. (2004 ▶); Janczak & Perpétuo (2001a ▶,b ▶,c ▶, 2002 ▶, 2003 ▶, 2004 ▶); Li et al. (2005 ▶); Perpétuo & Janczak (2002 ▶); Zhang et al. (2004 ▶).

Experimental

Crystal data

2C3H7N6 +·HPO4 2−·3H2O M = 404.32 Triclinic, a = 6.767 (4) Å b = 10.548 (7) Å c = 12.497 (8) Å α = 91.865 (11)° β = 105.609 (10)° γ = 108.020 (9)° V = 810.3 (9) Å3 Z = 2 Mo Kα radiation μ = 0.24 mm−1 T = 296 K 0.30 × 0.25 × 0.20 mm

Data collection

Bruker SMART 1K CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2000 ▶) T min = 0.933, T max = 0.954 3823 measured reflections 2803 independent reflections 2027 reflections with I > 2σ(I) R int = 0.029

Refinement

R[F 2 > 2σ(F 2)] = 0.057 wR(F 2) = 0.178 S = 1.06 2803 reflections 274 parameters H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.33 e Å−3 Δρmin = −0.53 e Å−3 Data collection: SMART (Bruker, 2000 ▶); cell refinement: SAINT (Bruker, 2000 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 (Farrugia, 1997 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶). Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809054798/hb5248sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809054798/hb5248Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
2C3H7N6+·HPO42−·3H2OZ = 2
Mr = 404.32F(000) = 424
Triclinic, P1Dx = 1.657 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 6.767 (4) ÅCell parameters from 1970 reflections
b = 10.548 (7) Åθ = 2.5–28.0°
c = 12.497 (8) ŵ = 0.24 mm−1
α = 91.865 (11)°T = 296 K
β = 105.609 (10)°Block, colourless
γ = 108.020 (9)°0.30 × 0.25 × 0.20 mm
V = 810.3 (9) Å3
Bruker SMART 1K CCD diffractometer2803 independent reflections
Radiation source: fine-focus sealed tube2027 reflections with I > 2σ(I)
graphiteRint = 0.029
ω scansθmax = 25.1°, θmin = 2.1°
Absorption correction: multi-scan (SADABS; Bruker, 2000)h = −7→8
Tmin = 0.933, Tmax = 0.954k = −11→12
3823 measured reflectionsl = −14→7
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.057Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.178H atoms treated by a mixture of independent and constrained refinement
S = 1.06w = 1/[σ2(Fo2) + (0.0996P)2 + 0.520P] where P = (Fo2 + 2Fc2)/3
2803 reflections(Δ/σ)max = 0.003
274 parametersΔρmax = 0.33 e Å−3
0 restraintsΔρmin = −0.53 e Å−3
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.
xyzUiso*/UeqOcc. (<1)
C10.5323 (6)0.7920 (4)−0.0156 (3)0.0352 (8)
C20.6740 (6)0.8584 (4)0.1714 (3)0.0359 (8)
C30.4373 (6)0.6393 (4)0.1008 (3)0.0337 (8)
C40.0847 (5)0.8128 (3)0.0751 (3)0.0317 (8)
C50.2296 (6)0.8597 (4)0.2627 (3)0.0372 (8)
C6−0.0212 (5)0.6489 (4)0.1803 (3)0.0329 (8)
N10.4191 (5)0.6664 (3)−0.0031 (2)0.0352 (7)
N20.6575 (5)0.8903 (3)0.0688 (2)0.0355 (7)
N30.5651 (5)0.7323 (3)0.1889 (3)0.0363 (7)
H30.577 (6)0.712 (4)0.248 (3)0.029 (10)*
N40.5233 (5)0.8212 (3)−0.1176 (3)0.0436 (8)
H4A0.59550.9002−0.12800.052*
H4B0.44530.7613−0.17410.052*
N50.7957 (5)0.9458 (3)0.2586 (3)0.0459 (8)
H5A0.86721.02580.24990.055*
H5B0.80470.92350.32490.055*
N60.3325 (5)0.5192 (3)0.1207 (3)0.0418 (8)
H6A0.25150.45770.06590.050*
H6B0.34500.50210.18860.050*
N70.2203 (5)0.9023 (3)0.1634 (2)0.0358 (7)
N80.1115 (5)0.7333 (3)0.2726 (3)0.0374 (7)
H80.126 (5)0.703 (3)0.334 (3)0.021 (8)*
N9−0.0400 (4)0.6864 (3)0.0791 (2)0.0330 (7)
N100.3541 (5)0.9350 (4)0.3562 (3)0.0552 (10)
H10A0.43431.01570.35500.066*
H10B0.35580.90390.41910.066*
N11−0.1322 (5)0.5270 (3)0.1931 (3)0.0420 (8)
H11A−0.21780.47090.13540.050*
H11B−0.11930.50310.25910.050*
N120.0741 (5)0.8512 (3)−0.0246 (2)0.0379 (7)
H12A0.15200.9305−0.03100.045*
H12B−0.01070.7969−0.08340.045*
P10.24796 (15)0.68587 (9)0.57240 (7)0.0335 (3)
O10.0294 (5)0.6330 (3)0.6053 (3)0.0599 (9)
H1−0.04820.56140.56690.090*
O2A0.2963 (6)0.8336 (3)0.5671 (3)0.0445 (14)0.767 (9)
O3A0.2088 (7)0.6098 (4)0.4601 (4)0.0353 (15)0.757 (14)
O4A0.4058 (6)0.6486 (5)0.6643 (3)0.0507 (16)0.765 (11)
O2B0.176 (2)0.7686 (13)0.4856 (10)0.046 (5)0.233 (9)
O3B0.279 (2)0.5614 (14)0.5130 (13)0.040 (5)0.243 (14)
O4B0.4481 (19)0.7567 (17)0.6642 (10)0.048 (5)0.235 (11)
O50.4731 (5)0.4107 (3)0.6295 (3)0.0606 (9)
H5C0.44050.47920.60780.091*
H5D0.57570.40630.60410.091*
O60.8660 (5)0.7583 (4)0.7442 (3)0.0753 (11)
H6C0.72990.74310.71890.113*
H6D0.89840.70380.70610.113*
O70.8612 (6)0.8583 (4)0.4724 (3)0.0799 (11)
H7A0.73200.80590.44200.120*
H7B0.94180.80930.48090.120*
U11U22U33U12U13U23
C10.0292 (18)0.040 (2)0.040 (2)0.0123 (16)0.0150 (15)0.0077 (16)
C20.0342 (19)0.039 (2)0.042 (2)0.0175 (16)0.0177 (16)0.0081 (17)
C30.0292 (18)0.038 (2)0.040 (2)0.0133 (15)0.0165 (15)0.0067 (16)
C40.0274 (18)0.039 (2)0.0343 (19)0.0133 (15)0.0146 (15)0.0090 (15)
C50.0281 (18)0.047 (2)0.035 (2)0.0074 (16)0.0143 (15)0.0034 (16)
C60.0272 (18)0.044 (2)0.0321 (19)0.0140 (16)0.0127 (14)0.0088 (15)
N10.0342 (17)0.0360 (17)0.0369 (17)0.0086 (13)0.0161 (13)0.0076 (13)
N20.0348 (16)0.0349 (17)0.0402 (17)0.0088 (13)0.0193 (13)0.0082 (13)
N30.0397 (18)0.0396 (18)0.0358 (19)0.0147 (14)0.0188 (15)0.0119 (15)
N40.0468 (19)0.0413 (18)0.0375 (18)0.0038 (15)0.0161 (14)0.0071 (14)
N50.054 (2)0.0432 (19)0.0371 (18)0.0088 (15)0.0154 (15)0.0043 (15)
N60.0464 (19)0.0408 (19)0.0396 (18)0.0101 (15)0.0188 (15)0.0120 (14)
N70.0302 (16)0.0381 (17)0.0375 (17)0.0053 (13)0.0146 (13)0.0040 (13)
N80.0384 (18)0.047 (2)0.0266 (17)0.0108 (15)0.0130 (14)0.0108 (14)
N90.0303 (15)0.0344 (17)0.0331 (16)0.0065 (13)0.0119 (12)0.0084 (12)
N100.048 (2)0.062 (2)0.0367 (19)−0.0071 (17)0.0125 (16)−0.0012 (16)
N110.0438 (18)0.0413 (18)0.0323 (17)0.0017 (14)0.0111 (14)0.0125 (13)
N120.0408 (18)0.0368 (17)0.0337 (17)0.0056 (14)0.0150 (13)0.0101 (13)
P10.0332 (5)0.0360 (5)0.0311 (5)0.0064 (4)0.0142 (4)0.0090 (4)
O10.0576 (19)0.0512 (19)0.068 (2)−0.0043 (14)0.0431 (16)−0.0138 (15)
O2A0.047 (2)0.039 (2)0.047 (3)0.0066 (17)0.022 (2)0.0108 (18)
O3A0.036 (2)0.037 (2)0.033 (2)0.0065 (16)0.0155 (18)0.0097 (17)
O4A0.058 (3)0.059 (4)0.038 (2)0.028 (2)0.0091 (17)0.0085 (18)
O2B0.060 (9)0.058 (9)0.030 (8)0.032 (7)0.015 (7)0.015 (6)
O3B0.042 (7)0.045 (8)0.039 (9)0.019 (6)0.015 (6)−0.006 (6)
O4B0.039 (7)0.054 (12)0.047 (7)0.012 (6)0.008 (5)0.011 (6)
O50.073 (2)0.075 (2)0.065 (2)0.0440 (18)0.0458 (17)0.0388 (16)
O60.065 (2)0.121 (3)0.0487 (19)0.050 (2)0.0113 (16)−0.0150 (18)
O70.085 (3)0.086 (3)0.077 (2)0.036 (2)0.025 (2)0.037 (2)
C1—N41.311 (5)N6—H6A0.8600
C1—N21.346 (5)N6—H6B0.8600
C1—N11.347 (5)N8—H80.84 (3)
C2—N51.303 (5)N10—H10A0.8600
C2—N21.320 (5)N10—H10B0.8600
C2—N31.363 (5)N11—H11A0.8600
C3—N61.315 (5)N11—H11B0.8600
C3—N11.320 (4)N12—H12A0.8600
C3—N31.347 (5)N12—H12B0.8600
C4—N121.313 (4)P1—O4B1.480 (12)
C4—N71.343 (5)P1—O2B1.488 (10)
C4—N91.350 (4)P1—O2A1.498 (4)
C5—N101.305 (5)P1—O4A1.498 (4)
C5—N71.326 (5)P1—O3A1.510 (4)
C5—N81.355 (5)P1—O11.581 (3)
C6—N111.313 (5)P1—O3B1.584 (11)
C6—N91.323 (4)O1—H10.8200
C6—N81.346 (5)O5—H5C0.8501
N3—H30.77 (4)O5—H5D0.8500
N4—H4A0.8600O6—H6C0.8500
N4—H4B0.8600O6—H6D0.8501
N5—H5A0.8600O7—H7A0.8508
N5—H5B0.8600O7—H7B0.8500
N4—C1—N2116.9 (3)H6A—N6—H6B120.0
N4—C1—N1118.0 (3)C5—N7—C4115.4 (3)
N2—C1—N1125.1 (3)C6—N8—C5119.8 (3)
N5—C2—N2121.1 (3)C6—N8—H8118 (2)
N5—C2—N3118.1 (3)C5—N8—H8122 (2)
N2—C2—N3120.7 (3)C6—N9—C4115.6 (3)
N6—C3—N1120.4 (3)C5—N10—H10A120.0
N6—C3—N3118.3 (3)C5—N10—H10B120.0
N1—C3—N3121.3 (3)H10A—N10—H10B120.0
N12—C4—N7117.0 (3)C6—N11—H11A120.0
N12—C4—N9116.9 (3)C6—N11—H11B120.0
N7—C4—N9126.1 (3)H11A—N11—H11B120.0
N10—C5—N7122.6 (4)C4—N12—H12A120.0
N10—C5—N8115.9 (3)C4—N12—H12B120.0
N7—C5—N8121.5 (3)H12A—N12—H12B120.0
N11—C6—N9120.4 (3)O4B—P1—O2B116.0 (8)
N11—C6—N8118.1 (3)O2A—P1—O4A115.2 (3)
N9—C6—N8121.5 (3)O2A—P1—O3A112.0 (2)
C3—N1—C1116.4 (3)O4A—P1—O3A112.0 (3)
C2—N2—C1116.6 (3)O4B—P1—O1116.8 (5)
C3—N3—C2119.9 (3)O2B—P1—O197.5 (5)
C3—N3—H3118 (3)O2A—P1—O1107.06 (18)
C2—N3—H3122 (3)O4A—P1—O1102.7 (2)
C1—N4—H4A120.0O3A—P1—O1106.93 (17)
C1—N4—H4B120.0O4B—P1—O3B109.3 (8)
H4A—N4—H4B120.0O2B—P1—O3B108.8 (9)
C2—N5—H5A120.0O1—P1—O3B107.7 (4)
C2—N5—H5B120.0P1—O1—H1109.5
H5A—N5—H5B120.0H5C—O5—H5D107.7
C3—N6—H6A120.0H6C—O6—H6D107.7
C3—N6—H6B120.0H7A—O7—H7B106.2
N6—C3—N1—C1−179.9 (3)N10—C5—N7—C4179.9 (4)
N3—C3—N1—C1−0.9 (5)N8—C5—N7—C41.0 (5)
N4—C1—N1—C3177.9 (3)N12—C4—N7—C5−179.0 (3)
N2—C1—N1—C3−1.1 (5)N9—C4—N7—C50.1 (5)
N5—C2—N2—C1178.3 (3)N11—C6—N8—C5179.6 (3)
N3—C2—N2—C1−1.1 (5)N9—C6—N8—C5−0.2 (5)
N4—C1—N2—C2−176.9 (3)N10—C5—N8—C6−180.0 (3)
N1—C1—N2—C22.1 (5)N7—C5—N8—C6−1.0 (5)
N6—C3—N3—C2−179.2 (3)N11—C6—N9—C4−178.6 (3)
N1—C3—N3—C21.8 (5)N8—C6—N9—C41.2 (5)
N5—C2—N3—C3179.9 (3)N12—C4—N9—C6178.0 (3)
N2—C2—N3—C3−0.8 (5)N7—C4—N9—C6−1.2 (5)
D—H···AD—HH···AD···AD—H···A
N3—H3···O5i0.77 (4)2.06 (4)2.791 (4)158 (4)
N4—H4B···O4Aii0.862.222.998 (5)151
N4—H4A···N7iii0.862.203.059 (5)177
N5—H5B···O70.861.972.822 (5)170
N5—H5A···O6iv0.862.413.258 (5)167
N6—H6B···O5i0.862.283.009 (5)143
N6—H6A···N9v0.862.173.031 (5)176
N8—H8···O3A0.84 (3)1.93 (4)2.742 (7)164 (3)
N10—H10B···O2A0.862.112.952 (5)168
N10—H10A···O2Avi0.861.992.744 (5)146
N11—H11B···O4Avii0.862.533.147 (6)129
N11—H11B···O1vii0.862.333.121 (5)152
N11—H11A···N1v0.862.022.884 (4)178
N12—H12B···O6viii0.862.072.840 (5)149
N12—H12A···N2iii0.862.082.935 (4)172
O1—H1···O3Avii0.821.762.535 (5)157
O5—H5D···O3Ai0.851.892.739 (5)177
O5—H5C···O4A0.852.002.726 (6)142
O6—H6D···O1ix0.851.972.787 (4)161
O6—H6C···O4A0.852.022.838 (6)162
O7—H7B···O1ix0.852.573.257 (5)139
O7—H7B···O2Aix0.852.282.958 (6)137
O7—H7A···O5i0.852.283.006 (6)144
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
N3—H3⋯O5i0.77 (4)2.06 (4)2.791 (4)158 (4)
N4—H4B⋯O4Aii0.862.222.998 (5)151
N4—H4A⋯N7iii0.862.203.059 (5)177
N5—H5B⋯O70.861.972.822 (5)170
N5—H5A⋯O6iv0.862.413.258 (5)167
N6—H6B⋯O5i0.862.283.009 (5)143
N6—H6A⋯N9v0.862.173.031 (5)176
N8—H8⋯O3A0.84 (3)1.93 (4)2.742 (7)164 (3)
N10—H10B⋯O2A0.862.112.952 (5)168
N10—H10A⋯O2Avi0.861.992.744 (5)146
N11—H11B⋯O4Avii0.862.533.147 (6)129
N11—H11B⋯O1vii0.862.333.121 (5)152
N11—H11A⋯N1v0.862.022.884 (4)178
N12—H12B⋯O6viii0.862.072.840 (5)149
N12—H12A⋯N2iii0.862.082.935 (4)172
O1—H1⋯O3Avii0.821.762.535 (5)157
O5—H5D⋯O3Ai0.851.892.739 (5)177
O5—H5C⋯O4A0.852.002.726 (6)142
O6—H6D⋯O1ix0.851.972.787 (4)161
O6—H6C⋯O4A0.852.022.838 (6)162
O7—H7B⋯O1ix0.852.573.257 (5)139
O7—H7B⋯O2Aix0.852.282.958 (6)137
O7—H7A⋯O5i0.852.283.006 (6)144

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) ; (viii) ; (ix) .

  10 in total

1.  Catena-poly[[diaqua(nicotinato-kappa2O,O')cadmium(II)]-mu-nicotinato-kappa3N:O,O'].

Authors:  Jian Zhang; Zhao Ji Li; Yi Hang Wen; Yao Kang; Ye Yan Qin; Yuan Gen Yao
Journal:  Acta Crystallogr C       Date:  2004-07-21       Impact factor: 1.172

2.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

3.  Melaminium acetate acetic acid solvate monohydrate.

Authors:  Genivaldo Julio Perpétuo; Jan Janczak
Journal:  Acta Crystallogr C       Date:  2002-01-23       Impact factor: 1.172

4.  Bis(melaminium) sulfate dihydrate.

Authors:  J Janczak; G J Perpétuo
Journal:  Acta Crystallogr C       Date:  2001-12-06       Impact factor: 1.172

5.  Melaminium chloride hemihydrate.

Authors:  J Janczak; G J Perpétuo
Journal:  Acta Crystallogr C       Date:  2001-09-11       Impact factor: 1.172

6.  Melaminium phthalate.

Authors:  J Janczak ; G J Perpétuo
Journal:  Acta Crystallogr C       Date:  2001-01       Impact factor: 1.172

7.  Cocrystallization of melaminium levulinate monohydrate.

Authors:  Chan Soo Choi; Ramaiyer Venkatraman; Eun Hee Kim; Hae Sook Hwang; Sung Kwon Kang
Journal:  Acta Crystallogr C       Date:  2004-03-31       Impact factor: 1.172

8.  Melaminium maleate monohydrate.

Authors:  Jan Janczak; Genivaldo Julio Perpétuo
Journal:  Acta Crystallogr C       Date:  2004-02-19       Impact factor: 1.172

9.  Bis(melaminium) DL-malate tetrahydrate.

Authors:  Jan Janczak; Genivaldo Julio Perpétuo
Journal:  Acta Crystallogr C       Date:  2003-05-31       Impact factor: 1.172

10.  Hexakis(melaminium) tetrakis(dihydrogenphosphate) monohydrogenphosphate tetrahydrate.

Authors:  Jan Janczak; Genivaldo Julio Perpétuo
Journal:  Acta Crystallogr C       Date:  2002-07-12       Impact factor: 1.172
  10 in total
  1 in total

1.  Crystal structure of bis-(2-amino-anilinium) hydrogen phosphate.

Authors:  Reena Ittyachan; Melesuparambil Sundaram Ahigna; Rajamony Jagan
Journal:  Acta Crystallogr E Crystallogr Commun       Date:  2016-03-22
  1 in total

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